Method for determining fluid contents of solids



Oct. 31, 1944. w. L. HORNER METHOD FOR DETERMINING FLUID CONTENTS OF SOLIDS Original Filed Jan. 5, 1938 wmwi WW-WM INVENTOR Wzllzam l -H0rner NYS Patented Oct. 31, 1944 1 METHOD FOR DETERMINING FLUID CONTENTS OF SOLIDS William L. Horner, Dallas, 'I'ex., assignor toGore Laboratories, Inc., Dallas, Tex., a corporation of Delaware Original application January 3, 1938, Serial No.

* 183,018, now Patent No. 2,296,852, dated September 29, 1942. Divided and this application December 27, 1941, Serial No. 424,588

1 Claim.

In one embodiment of the present invention core samples are placed in a chamber. The sample is heated to vaporize liquids present in the pores of the sample. The vapors are drawn a downwardly through ,and in contact with the core sample and are discharged from the chamber in such manner that the vapors leave the chamber in a region which is cooler than the region in which they were distilled. The vapors are condensed and collected in a suitable measuring container.

If both oil and water are present in the sample, the amount of water that is present as free water in contrast to the water whichmay be considered 1 as water of crystallization is determined by plotting the water collected against time so that the amount of water collected at any interval of time may be determined. Since the free water is distilled oil wit greater ease and at lower temperatures than 5 the water of crystallization,

: and so is distilled oif before the. water of crystallization is distilled off, the amount of free water may be determined by noting the total amount of water collected at the time water condensate first stops collecting in the container.

The still shown in th drawing is adapted to distill oil and water from core samples S and to collect the products of distillation in a graduated tube generally indicated at 2 supported below tlzestill by a connecting tube generally indicated a The still comprises an insulated heater having an inner chamber 6 adapted to receive a sample container 8. Around chamber 6 is a ceramic shell, such as porcelain, and indicated at Ill. The shell is spirally grooved on its outside as shown and is open at its bottom and is closed at its top with a porcelain top l2. Closely fitted inside the porcelain shell ,is located a polished steel shell l4 having sides, and a top and sup- Wound around the outside of the grooved porcelain shell is a resistance heating wire 18, and packed around this wire and held in by a suitable metal cover is suitable packing 22, such as magnesium silicate. The top and bottom walls holding the magnesium-silicate packing are respectively an asbestos disc 24 and an annular ring 26, held together by three tie lrods 28. The ends of the resistance wire come out through the top 24 and are securedto suitable insulated terminals 30 from which extends a cord adapted to connect the resistance wire with a supply of electricity. As shown in the drawing, the heating mechanism does not extend to the lower part ofthe steel shell l4 and consequently the lowar portion of the shell and the bottom 34 are not heated to the temperatures to which the upper parts of the apparatus are heated.

The annular supporting flange I6 is provided with downwardly-extending bolts 32 for clamping a base plate 34 to the supporting flange.

,'The inside of the base plate is conically dished at its center, as shown, and at the apex of the conical formation is provided an outlet 36 into rubber stopper which is brazed a short bronze tube 38. The outlet tube is connected by suitable rubber connections to a tlatively long copper tube l4!) serving as'a co denser and terminating in a 2 in the top of the, graduated glass tube 2. A suitable vent 44 also extends up: wardly from th stopper. f

The sample ontainer 8 is preferably made of some corrosion resisting material, such as monel metal, or is plated with some corrosion resisting plating. It is open at its top and has a perforated bottom. 1 A spacing rod 46 extends downvv'ardly from thecontainer.

In operation the sample container is filled with and is pushed to the top o f the chamber by the spacing rod 48 as the base Q4 is moved into its closing position. After thecontainer and sample have been placed in the heating chamber 6v and the base plate 34 bolted in place, the heat is turned on and the sample is eventually heated to a dull, red temperature which insures all oil, gas

, and water being driven off. The oil, which is so ported at its open bot torn by a flange ring i6.

driven off in the form of vapors, is always caused to move to cooler regions, and as it passes down through the tube! is sufficiently cooledpjo that it condenses and drips into the graduate tube 2.

During the heating, the amount of oil and water collecting in the tube is plotted against time, because the first water that comes off is the free water, i. e., the connate water and drillmud waterwhich may be present in the sample.

As the heating continues, the water stops coming over for a short time and then commences to come over again. This last water to come over is probably water of crystallization and does not enter into the problem of oil production. The purpose of plotting the water distilled against time is to be able to read the amount of total free water distilled from the sample. From the graduations on the tube 2 is obtained the amount of oil that came over and the amount of total water. The weight measurement of the sample put into the chamber 8 may be converted to volume by means of a density measurement made by weighing a corresponding sample and obtaining the volume of the sample by a liquid displacement measurement. Thus from the foregoing readings it is possible to obtain the percentage of oil saturation and the percentage of total water saturation per unit volume of core sample.

The above method of distilling the water and oil from the sample has the advantage of being rapid and accurate. The heavy vapors of the distillate flow by gravity to the colder regions and the condensing tube. A further advantage of the present method is that the heating of the sample is carried out uniformly so that the sample of water obtained is free from water of crystallization and the sample of oil obtained represents practically 98% recovery.

As various embodiments might be made of this invention, all without departing from the scope of the invention, it is to be understood that all matter herein set forth or shown in the accompanying drawing is to be interpreted as illustrative and. not in a limiting sense.

I claim:

In the process of determining the oil and free water content of a core sample, the steps of supplying heat energy at a constant rate to a chamber containing the sample to distill oil the oil and water from the sample, causing the water and oil vapors to move downwardly through and in contact with the sample in said chamber and to pass downwardly from the bottom of said chamber, moving always to a cooler region; condensing the vapors thus removed from the sample, measuring the amount of water condensate at predetermined intervals of time to determine the amount of free water distilled from the sample by noting the amount of water condensate at the interval of time when it first stops distilling of! and measuring the total amount of 011 condensed to obtain the amount of oil distilled from thesample.

WILLIAM L. HORNER. 

